CN107255626A - 一种淀粉基油炸食品中油脂含量的快速测定方法 - Google Patents
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Abstract
本发明公开了一种淀粉基油炸食品中油脂含量的快速测定方法,所述测定方法包括如下具体步骤:(1)对已知油脂浓度的标准溶液进行红外光谱检测;(2)以谱图中1743cm‑1处油脂分子酯键的特征峰作为定量依据,将油脂含量与特征峰积分面积建立线性回归方程;(3)待测样品检测前经过预处理;(4)采用步骤(1)的方法对待测样品进行红外光谱检测,将红外图谱中1743cm‑1处油脂分子酯键的特征峰积分面积代入回归方程,计算得到待测样品的油脂含量。本发明方法能够实现测试过程的统一化、规范化,对于淀粉基油炸食品品质监控、油炸工艺改良、产品配方优化、油脂含量控制等具有重要的现实意义。
Description
技术领域
本发明涉及油脂检测的技术领域,尤其是涉及一种通过衰减全反射-傅立叶变换红外光谱快速测定淀粉基油炸食品中油脂含量的方法。
背景技术
油炸食品在食品工业、餐饮业仍至老百姓的一日三餐中占据重要地位,无论是逢年过节的炸麻花、炸春卷,还是每天早餐所食用的油条、面窝、麻团;儿童喜欢食用的洋快餐中的炸鸡腿、炸面包及零食里的方便面、薯片等,无一不是油炸食品,可以说我们天天都在和油炸食品打交道。油炸食品含有较多的油脂,有些油炸食品中油脂质量达到食物质量的1/3。食物中吸收的油脂在增强人们饱腹感、提高营养价值的同时,也产生了一个严重的问题,即油脂的过量摄入导致的健康问题。因此,油脂含量的高效、快速测定,成为了油炸食品品质控制、工艺改进的重要前提。
目前,常规的脂类含量测定方法如索氏抽提法,存在耗时长、稳定性差、易受干扰等缺陷,并不能满足工业生产中大批量样品检测分析的要求。
发明内容
本发明的技术方案如下:
针对现有技术存在的问题,本发明申请人提供了一种淀粉基油炸食品中油脂含量的快速测定方法。本发明所提出的油脂含量测定新方法,主要基于油脂分子红外光谱中1743cm-1处对应于油脂特征官能团-COO的吸收峰,且该峰并不受部分有机溶剂红外吸收峰的干扰,可作为脂类物质的指纹特征用于油脂分子的定性、定量分析。
本发明方法能够实现测试过程的统一化、规范化,且易于在油炸食品工业中进行推广应用,对于淀粉基油炸食品品质监控、油炸工艺改良、产品配方优化、油脂含量控制等具有重要的现实意义。
一种淀粉基油炸食品中油脂含量的快速测定方法,所述测定方法包括如下具体步骤:
(1)对已知油脂浓度的标准溶液进行红外光谱检测;
(2)以步骤(1)的检测谱图中1743cm-1处油脂分子酯键的特征峰作为定量依据,将油脂含量与特征峰积分面积建立线性回归方程;
(3)待测样品检测前经过预处理;
(4)采用步骤(1)的方法对预处理的待测样品进行红外光谱检测,将待测样品红外图谱中1743cm-1处油脂分子酯键的特征峰积分面积代入回归方程,计算得到待测样品的油脂含量。
所述红外光谱检测所用设备为衰减全反射-傅里叶变换红外光谱仪,型号IS10,美国Nicolet公司生产。
所述红外光谱检测的条件为:扫描范围600-4000cm-1、扫描次数32次、分辨率4cm-1;经大气背景扣除、基线校正处理后,选定1693-1793cm-1范围对1743cm-1处油脂分子特征官能团吸收峰进行积分。
步骤(1)中所述标准溶液的质量浓度为0.5-70%,溶质为大豆油、棕榈油、玉米油、菜籽油、稻米油中的一种或多种,溶剂为正己烷、环己烷、二甲亚砜、三氯甲烷、乙醇中的任何一种。
步骤(2)中所述线性回归方程为:将系列油脂标准样品的油脂浓度与其对应红外光谱中1743cm-1油脂分子特征官能团吸收峰积分面积进行相关性分析,得到一元线性回归方程y=ax+b,其中y为系列油脂标准样品在1743cm-1处对应油脂分子酯键的特征峰积分面积,x为油脂浓度,a和b分别为标准曲线的斜率和截距。
步骤(3)中所述预处理的方法为:(1)准确称取定量待测淀粉基油炸食品于玛瑙研钵中,充分研磨粉碎,将经粉碎的样品分散于正己烷、环己烷、二甲亚砜、三氯甲烷、乙醇中的任何一种中,制得待测样品分散液;(2)取20-50μL样品分散液,均匀涂布于ATR-FTIR专用测试平台上,需确保测试台上样品液膜的厚度不超过5μm。
本发明的有益成果在于:
本发明方法具有灵敏度高、重复性好、准确度高、操作简单等明显优势,能够实现测试过程的统一化、规范化,且易于在油炸食品工业中进行推广应用,对于淀粉基油炸食品品质监控、油炸工艺改良、产品配方优化、油脂含量控制等具有重要的现实意义。
传统索氏抽提法测定脂肪含量需要耗时12-24小时,且测定全程均需通以冷水进行冷却,还需要不断补充消耗的有机试剂,测试过程对环境有一定污染,繁琐的过程使得该法不适合大量样品的分析测定;索氏抽提法需要的样品量也比较多,通常需要2-3g,如果样品含油量较低,则需要更多的样品;此外索氏抽提法测定结果还受样品中其他成分的影响,如在用乙醚作为提取剂时,样品中残留水分会显著降低乙醚对脂类物质的溶解,部分油脂会与食品结构紧密结合在一起,不利于溶剂对脂类物质的充分提取,也会影响测定结果的准确性。
本发明方法利用油脂分子红外光谱中1743cm-1处对应于的油脂特征官能团-COO-吸收峰,其不受部分有机溶剂红外吸收峰干扰,可用于油脂分子的定性、定量分析。该法测定过程简便快速,一个样品仅需2-5分钟即可完成测定;本方法需要的样品量很少,10-50mg样品即可;本方法的灵敏度较高,即使样品中的含油量低于5%,用少量样品也可以准确测定。
附图说明
图1为本发明示意图;
图2为实施例1中系列油脂标准样品ATR-FTIR图谱;
图3为实施例1中油脂标准曲线;
图4为实施例1中淀粉基油炸样品的ATR-FTIR图谱。
具体实施方式
下面结合附图和实施例,对本发明进行具体描述。
实施例1
一种淀粉基油炸食品中油脂含量的快速测定方法,所述测定方法包括如下具体步骤:
(1)对已知油脂浓度的标准溶液进行红外光谱检测:
精密称量一定质量的大豆油,溶于正己烷中配成浓度为1.01%,4.93%,19.93%,40.00%的系列标准溶液;然后在扫描范围600-4000cm-1、扫描次数32次、分辨率4cm-1的红外检测条件下得到一系列的红外谱图,如图2所示,求出1743cm-1处油脂分子酯键的特征峰积分面积,结果如表1所示;
(2)以步骤(1)的检测谱图中1743cm-1处油脂分子酯键的特征峰作为定量依据,发现1743cm-1处酯键特征峰面积与油脂含量成正比,所以将油脂含量与特征峰积分面积建立线性回归方程,如图3所示;
回归方程为:y=0.0726x+0.0795(R2=0.9976)
(3)待测样品检测前经过预处理:
将新鲜马铃薯切成厚度为5mm薄片,置于180℃油炸锅中用大豆油油炸处理5min,油炸完毕,取出油炸马铃薯片,沥油后置于密封袋中待测;
准确称取50mg油炸马铃薯片于玛瑙研钵中,充分研磨粉碎,将经粉碎的样品充分分散于正己烷中,取50μL样品分散液,均匀涂布于ATR-FTIR专用测试平台上,需确保测试台上样品液膜的厚度不超过5μm。
(4)采用步骤(1)的方法对预处理的待测样品进行红外光谱检测,红外图谱如图4所示,淀粉基油炸样品红外图谱主要由淀粉的红外信号与油脂的红外信号叠加而成,其中1743cm-1处油脂分子中酯键特征峰很强,且与淀粉红外信号区分度较高,将待测样品红外图谱中1743cm-1处油脂分子酯键的特征峰积分面积代入回归方程,计算得到待测样品的油脂含量。
测定出上述油炸条件下样品中油脂含量为0.39%,与索氏抽提法相比,结果偏差小于2%。
表1
实施例2
一种淀粉基油炸食品中油脂含量的快速测定方法,所述测定方法包括如下具体步骤:
(1)对已知油脂浓度的标准溶液进行红外光谱检测:
精密称量一定质量的棕榈油,溶于正己烷中配成浓度为2.61%,7.48%,30.00%,60.02%的系列标准溶液;然后在扫描范围600-4000cm-1、扫描次数32次、分辨率4cm-1的红外检测条件下得到一系列的红外谱图,求出1743cm-1处油脂分子酯键的特征峰积分面积,结果如表2所示;
(2)以步骤(1)的检测谱图中1743cm-1处油脂分子酯键的特征峰作为定量依据,将油脂含量与特征峰积分面积建立线性回归方程;
回归方程为:y=0.0730x+0.0448(R2=0.9988)
(3)待测样品检测前经过预处理:
将新鲜马铃薯切成厚度为10mm薄片,置于180℃油炸锅中用棕榈油炸处理3min,油炸完毕,取出油炸马铃薯片,沥油后置于密封袋中待测;
准确称取50mg油炸马铃薯片于玛瑙研钵中,充分研磨粉碎,将经粉碎的样品充分分散于正己烷中,取50μL样品分散液,均匀涂布于ATR-FTIR专用测试平台上,需确保测试台上样品液膜的厚度不超过5μm。
(4)采用步骤(1)的方法对预处理的待测样品进行红外光谱检测,将待测样品红外图谱中1743cm-1处油脂分子酯键的特征峰积分面积代入回归方程,计算得到待测样品的油脂含量。
测定出上述油炸条件下样品中油脂含量为0.43%,与索氏抽提法相比,结果偏差小于2%。
表2
实施例3
一种淀粉基油炸食品中油脂含量的快速测定方法,所述测定方法包括如下具体步骤:
(1)对已知油脂浓度的标准溶液进行红外光谱检测:
精密称量一定质量的玉米油,溶于正己烷中配成浓度为0.57%,10.00%,50.00%,70.00%的系列标准溶液;然后在扫描范围600-4000cm-1、扫描次数32次、分辨率4cm-1的红外检测条件下得到一系列的红外谱图,求出1743cm-1处油脂分子酯键的特征峰积分面积,结果如表3所示;
(2)以步骤(1)的检测谱图中1743cm-1处油脂分子酯键的特征峰作为定量依据,将油脂含量与特征峰积分面积建立线性回归方程;
回归方程为:y=0.0709x+0.0607(R2=0.9986)
(3)待测样品检测前经过预处理:
将新鲜马铃薯切成厚度为5mm薄片,置于150℃油炸锅中用玉米油炸处理2min,油炸完毕,取出油炸马铃薯片,沥油后置于密封袋中待测;
准确称取50mg油炸马铃薯片于玛瑙研钵中,充分研磨粉碎,将经粉碎的样品充分分散于正己烷中,取50μL样品分散液,均匀涂布于ATR-FTIR专用测试平台上,需确保测试台上样品液膜的厚度不超过5μm。
(4)采用步骤(1)的方法对预处理的待测样品进行红外光谱检测,将待测样品红外图谱中1743cm-1处油脂分子酯键的特征峰积分面积代入回归方程,计算得到待测样品的油脂含量。
测定出上述油炸条件下样品中油脂含量为0.48%。与索氏抽提法相比,结果偏差小于2%。
表3
Claims (6)
1.一种淀粉基油炸食品中油脂含量的快速测定方法,其特征在于所述测定方法包括如下具体步骤:
(1)对已知油脂浓度的标准溶液进行红外光谱检测;
(2)以步骤(1)的检测谱图中1743cm-1处油脂分子酯键的特征峰作为定量依据,将油脂含量与特征峰积分面积建立线性回归方程;
(3)待测样品检测前经过预处理;
(4)采用步骤(1)的方法对预处理的待测样品进行红外光谱检测,将待测样品红外图谱中1743cm-1处油脂分子酯键的特征峰积分面积代入回归方程,计算得到待测样品的油脂含量。
2.根据权利要求1所述的测定方法,其特征在于所述红外光谱检测所用设备为衰减全反射-傅里叶变换红外光谱仪,型号IS10,美国Nicolet公司生产。
3.根据权利要求1所述的测定方法,其特征在于所述红外光谱检测的条件为:扫描范围600-4000cm-1、扫描次数32次、分辨率4cm-1;经大气背景扣除、基线校正处理后,选定1693-1793cm-1范围对1743cm-1处油脂分子特征官能团吸收峰进行积分。
4.根据权利要求1所述的测定方法,其特征在于步骤(1)中所述标准溶液的质量浓度为0.5-70%,溶质为大豆油、棕榈油、玉米油、菜籽油、稻米油中的一种或多种,溶剂为正己烷、环己烷、二甲亚砜、三氯甲烷、乙醇中的任何一种。
5.根据权利要求1所述的测定方法,其特征在于步骤(2)中所述线性回归方程为:将系列油脂标准样品的油脂浓度与其对应红外光谱中1743cm-1油脂分子特征官能团吸收峰积分面积进行相关性分析,得到一元线性回归方程y=ax+b,其中y为系列油脂标准样品在1743cm-1处对应油脂分子酯键的特征峰积分面积,x为油脂浓度,a和b分别为标准曲线的斜率和截距。
6.根据权利要求1所述的测定方法,其特征在于步骤(3)中所述预处理的方法为:
(1)准确称取定量待测淀粉基油炸食品于玛瑙研钵中,充分研磨粉碎,将经粉碎的样品分散于正己烷、环己烷、二甲亚砜、三氯甲烷、乙醇中的任何一种中,制得待测样品分散液;
(2)取20-50μL样品分散液,均匀涂布于ATR-FTIR专用测试平台上,需确保测试台上样品液膜的厚度不超过5μm。
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